US4375452A - Process for the separation and recovery of molybdenum and uranium from leach solution using ion exchange - Google Patents

Process for the separation and recovery of molybdenum and uranium from leach solution using ion exchange Download PDF

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US4375452A
US4375452A US06/311,579 US31157981A US4375452A US 4375452 A US4375452 A US 4375452A US 31157981 A US31157981 A US 31157981A US 4375452 A US4375452 A US 4375452A
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uranium
values
molybdenum
resin
eluate
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US06/311,579
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Raymond J. Jan
Alistair H. Montgomery
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Mobil Oil AS
ExxonMobil Oil Corp
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/0265—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries extraction by solid resins
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a process for recovering and separating uranium and molybdenum from a pregnant lixiviant by two-stage ion-exchange adsorption.
  • Uranium ore deposits which contain certain portions of other metals such as calcium, molybdenum etc. are selectively leached in-situ by passing through a relatively diluted carbonate/bicarbonate solution with oxidants such as oxygen and hydrogen peroxide.
  • the solution withdrawn from the ore deposits will then contain uranium and various contaminants in their different ionic forms co-produced during uranium leaching with molybdenum being the most persistant contaminant.
  • Uranium as well as molybdenum are recovered when the solution is brought into contact with a strong base anion-exchange resin which selectively adsorbs uranium and molybdenum.
  • separation of molybdenum from the uranium eluate can be accomplished by using a tertiary amine solvent at 3-3.5 pH.
  • Molybdenum can also be selectively loaded onto an activated charcoal column thus producing a Mo-free uranium eluant for recovery.
  • the present invention provides a process for the recovery of uranium from a pregnant lixiviant containing molybdenum as the primary contaminant using a two-stage ion-exchange recovery process.
  • a strong base anionic resin comprising a quaternary amine is employed in a primary column to adsorb uranium and molybdenum values from the pregnant lixiviant.
  • the uranium and molybdenum values loaded on the strong base anionic resin are then eluted from the resin with a suitable eluant such as a salt solution which may contain carbonate/bicarbonate.
  • the pregnant eluate containing uranium and molybdenum values is passed through a secondary column containing a weak acid cationic resin in its hydrogen form wherein the uranium values are adsorbed by the resin.
  • the resin in the secondary column is then treated with an acid eluant to recover the uranium values loaded on the resin.
  • the pregnant eluate containing uranium values free of molybdenum is then treated to precipitate uranium therefrom to produce the familiar "yellow-cake.
  • the FIGURE is a schematical view of an in-situ leaching circuit for the recovery of uranium from a pregnant lixiviant containing molybdenum as the most prominent contaminant utilizing a two-stage ion-exchange adsorption process in accordance with the present invention.
  • Uranium containing ore deposits are economically leached by a conventional leaching process wherein uranium values along with other contaminating values wherein molybdenum is the most prominent contaminant are extracted from the ore by means of a leaching fluid or lixiviant.
  • the leaching fluid or lixiviant is introduced into the ore deposit through a predetermined pattern of injection wells.
  • the lixiviant or leaching solution which may be acidic or alkaline depending on the nature of the ore, will preferentially dissolve uranium values along with a certain portion of contaminating molybdenum values.
  • the resulting uranium-enriched solution (pregnant lixiviant) with the uranium values computed as U 3 O 8 and also containing molybdenum values is then retrieved through a pattern of production wells for subsequent separation and recovery of the uranium and molybdenum values from the leach solution by means of the present invention involving a two-step ion-exchange resin process.
  • the pregnant lixiviant contains uranium and molybdenum values.
  • the pregnant U 3 O 8 .Mo lixiviant flows from the withdrawal well (not shown) in the well field via line 10 to a primary column 12 containing a strong base anionic resin comprising a quaternary amine.
  • the resin is made from a styrene divinyl benzene copolymer.
  • the reactive intermediate is prepared by chloromethylation of the solvent swollen copolymer beads.
  • the intermediate is capable of reacting with a wide variety of amines to produce anion exchange resins of varying chemical functional groups.
  • Resins useful in accordance with the present invention include the materials sold under the trademark Dowex 21K and MSA-1 by Dow Chemical Company and also Rohm & Haas Company's IRA-400.
  • uranium and molybdenum values are loaded on to the ion-exchange resin and the barren lixiviant, now stripped of the desired values, passes from the column via line 14 to a mixing tank 16 where desired amounts of chemicals such as sodium carbonate, carbon dioxide, oxidant, (not shown) are added to the barren lixiviant to brint it back up to strength for recycling in the wellfield leach circuit.
  • the uranium and molybdenum values are eluted from the ion-exchange resin in column 12 by passing an eluant comprising a salt solution which may contain carbonate/bicarbonate via line 20 through the column.
  • the uranium and molybdenum values are thus extracted from the ion-exchange resin in column 12 to provide a pregnant eluate containing these values that is withdrawn from the column via line 22.
  • the U 3 O 8 .Mo eluate is transported via line 22 and introduced into the secondary ion-exchange column 24 containing a weak acid cationic resin in hydrogen form. Because the resin in the secondary column 24 is in hydrogen form, the column is operated at an acidic pH.
  • a suitable major functional group may be selected from the group consisting of carboxylic acid, phenolic, phosphoric, and sulph-hydryl.
  • the U 3 O 8 .Mo eluate passes through the ion-exchange resin in column 24 and the uranium values are adsorbed by the resin and the stripped eluate containing molybdenum is withdrawn from the column via line 26.
  • the barren eluate is carried via line 26 to a molybdenum concentrating means 28.
  • the barren solution containing concentrated molybdenum is removed from concentrating means 28 via line 30 and into a separation means 32 where the molybdenum is separated from the liquid barren eluate and withdrawn via line 34.
  • the liquid barren eluate is passed to a mixing tank 36 via line 38 where it is adjusted or fortified with additional chemicals to bring it back up to strength for recycling into column 12 via line 20 to eluate U 3 O 3 .Mo therefrom.
  • the size of the secondary ion-exchange resin, column 24 is preferably smaller than that of the primary column 12.
  • An acid solution eluant such as 4% HCl or H 2 SO 4 is introduced into column 24 via line 40 to strip the molybdenum-free uranium values from the weak cationic resin.
  • the pregnant eluate containing uranium values is withdrawn from the column 24 via line 42 and pumped to vessel 44 for precipitation of the uranium values preferably by reacting the uranium values with hydrogen peroxide in an acid solution to form a hydrated uranium peroxide product, e.g., UO 4 ⁇ H 2 O or by treating the eluate with an acid and then with ammonia to precipitate ammonium diuranate.
  • the resulting precipitate, yellow-cake slurry is pumped to a storage tank 46 via line 48 for settling and decanting.
  • the barren solution is conveyed via line 50 to a mixing tank 52 where those chemicals being used to form the eluant used to recover the uranium from column 24 are added to the barren solution to bring it back up to strength for recycling via line 40 to the secondary ion-exchange column 24.
  • the yellow-cake slurry is withdrawn from tank 46 via line 54 and pumped to a vacuum dryer (not shown) where it is dried to yellow-cake powder.
  • the final uranium containing product is free of molybdenum.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A process is described for recovering uranium from a pregnant lixiviant containing uranium values and a certain portion of molybdenum values comprising passing the pregnant lixiviant through an anion-exchange resin to capture the uranium and molybdenum values on the resin, eluting the uranium and molybdenum values from the resin with a salt solution, passing the eluate through a weak acid cationic resin in its hydrogen form to capture the uranium values on the resin and treating and resulting eluate to precipitate uranium therefrom to produce the familiar "yellow-cake."

Description

BACKGROUND OF THE INVENTION
The present invention relates to a process for recovering and separating uranium and molybdenum from a pregnant lixiviant by two-stage ion-exchange adsorption.
Uranium ore deposits which contain certain portions of other metals such as calcium, molybdenum etc. are selectively leached in-situ by passing through a relatively diluted carbonate/bicarbonate solution with oxidants such as oxygen and hydrogen peroxide. The solution withdrawn from the ore deposits will then contain uranium and various contaminants in their different ionic forms co-produced during uranium leaching with molybdenum being the most persistant contaminant. Uranium as well as molybdenum are recovered when the solution is brought into contact with a strong base anion-exchange resin which selectively adsorbs uranium and molybdenum.
Since both uranium and molybdenum are loaded on the anionic resin, and in most cases eluted altogether (although their elution efficiency may be different), a purification step(s) is required before a Mo-free uranium is produced.
Various methods are used for countering the molybdenum problem involving either some method of removing molybdenum from the process liquors or of treating resins in ion exchange methods and solvents in solvent exchange methods to rid them of excess molybdenum.
For example, separation of molybdenum from the uranium eluate can be accomplished by using a tertiary amine solvent at 3-3.5 pH. Molybdenum can also be selectively loaded onto an activated charcoal column thus producing a Mo-free uranium eluant for recovery.
The process of the present invention offers simplicity and economics as compared to the prior art techniques.
SUMMARY OF THE INVENTION
The present invention provides a process for the recovery of uranium from a pregnant lixiviant containing molybdenum as the primary contaminant using a two-stage ion-exchange recovery process. In accordance with the first stage of the present invention, a strong base anionic resin comprising a quaternary amine is employed in a primary column to adsorb uranium and molybdenum values from the pregnant lixiviant. The uranium and molybdenum values loaded on the strong base anionic resin are then eluted from the resin with a suitable eluant such as a salt solution which may contain carbonate/bicarbonate. In the second stage of the process, the pregnant eluate containing uranium and molybdenum values is passed through a secondary column containing a weak acid cationic resin in its hydrogen form wherein the uranium values are adsorbed by the resin. The resin in the secondary column is then treated with an acid eluant to recover the uranium values loaded on the resin. Finally, the pregnant eluate containing uranium values free of molybdenum is then treated to precipitate uranium therefrom to produce the familiar "yellow-cake.
BRIEF DESCRIPTION OF THE DRAWING
The actual operation and the apparent advantages of the invention will be better understood by referring to the drawing in which:
The FIGURE is a schematical view of an in-situ leaching circuit for the recovery of uranium from a pregnant lixiviant containing molybdenum as the most prominent contaminant utilizing a two-stage ion-exchange adsorption process in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Uranium containing ore deposits are economically leached by a conventional leaching process wherein uranium values along with other contaminating values wherein molybdenum is the most prominent contaminant are extracted from the ore by means of a leaching fluid or lixiviant. In the case of in-situ leaching, the leaching fluid or lixiviant is introduced into the ore deposit through a predetermined pattern of injection wells. The lixiviant or leaching solution, which may be acidic or alkaline depending on the nature of the ore, will preferentially dissolve uranium values along with a certain portion of contaminating molybdenum values. The resulting uranium-enriched solution (pregnant lixiviant) with the uranium values computed as U3 O8 and also containing molybdenum values is then retrieved through a pattern of production wells for subsequent separation and recovery of the uranium and molybdenum values from the leach solution by means of the present invention involving a two-step ion-exchange resin process.
Referring to the drawing, a description of a preferred embodiment of the method of this invention will be given wherein the pregnant lixiviant contains uranium and molybdenum values. As shown in the drawing, the pregnant U3 O8.Mo lixiviant flows from the withdrawal well (not shown) in the well field via line 10 to a primary column 12 containing a strong base anionic resin comprising a quaternary amine. The resin is made from a styrene divinyl benzene copolymer. To introduce the functional group into the copolymer bead, it is necessary to produce a reactive intermediate. The reactive intermediate is prepared by chloromethylation of the solvent swollen copolymer beads. The intermediate is capable of reacting with a wide variety of amines to produce anion exchange resins of varying chemical functional groups. Resins useful in accordance with the present invention include the materials sold under the trademark Dowex 21K and MSA-1 by Dow Chemical Company and also Rohm & Haas Company's IRA-400. In the ion-exchange column 12, uranium and molybdenum values are loaded on to the ion-exchange resin and the barren lixiviant, now stripped of the desired values, passes from the column via line 14 to a mixing tank 16 where desired amounts of chemicals such as sodium carbonate, carbon dioxide, oxidant, (not shown) are added to the barren lixiviant to brint it back up to strength for recycling in the wellfield leach circuit.
The uranium and molybdenum values are eluted from the ion-exchange resin in column 12 by passing an eluant comprising a salt solution which may contain carbonate/bicarbonate via line 20 through the column. The uranium and molybdenum values are thus extracted from the ion-exchange resin in column 12 to provide a pregnant eluate containing these values that is withdrawn from the column via line 22. The U3 O8.Mo eluate is transported via line 22 and introduced into the secondary ion-exchange column 24 containing a weak acid cationic resin in hydrogen form. Because the resin in the secondary column 24 is in hydrogen form, the column is operated at an acidic pH. For the weak acid cationic resin, a suitable major functional group may be selected from the group consisting of carboxylic acid, phenolic, phosphoric, and sulph-hydryl. The U3 O8.Mo eluate passes through the ion-exchange resin in column 24 and the uranium values are adsorbed by the resin and the stripped eluate containing molybdenum is withdrawn from the column via line 26. The barren eluate is carried via line 26 to a molybdenum concentrating means 28. The barren solution containing concentrated molybdenum is removed from concentrating means 28 via line 30 and into a separation means 32 where the molybdenum is separated from the liquid barren eluate and withdrawn via line 34. The liquid barren eluate is passed to a mixing tank 36 via line 38 where it is adjusted or fortified with additional chemicals to bring it back up to strength for recycling into column 12 via line 20 to eluate U3 O3.Mo therefrom. The size of the secondary ion-exchange resin, column 24 is preferably smaller than that of the primary column 12.
An acid solution eluant such as 4% HCl or H2 SO4 is introduced into column 24 via line 40 to strip the molybdenum-free uranium values from the weak cationic resin. The pregnant eluate containing uranium values is withdrawn from the column 24 via line 42 and pumped to vessel 44 for precipitation of the uranium values preferably by reacting the uranium values with hydrogen peroxide in an acid solution to form a hydrated uranium peroxide product, e.g., UO4 ×H2 O or by treating the eluate with an acid and then with ammonia to precipitate ammonium diuranate. The resulting precipitate, yellow-cake slurry, is pumped to a storage tank 46 via line 48 for settling and decanting. Once the slurry is settled, the barren solution is conveyed via line 50 to a mixing tank 52 where those chemicals being used to form the eluant used to recover the uranium from column 24 are added to the barren solution to bring it back up to strength for recycling via line 40 to the secondary ion-exchange column 24. The yellow-cake slurry is withdrawn from tank 46 via line 54 and pumped to a vacuum dryer (not shown) where it is dried to yellow-cake powder. The final uranium containing product is free of molybdenum.
The foregoing description of my invention has been directed to particular details in accordance with the requirements of the Patent Act and for purposes of explanation and illustration. It will be apparent, however, to those skilled in this art that many modifications and changes may be made without departing from the scope and spirit of the invention. It is further apparent that persons of ordinary skill in this art will, on the basis of this disclosure, be able to practice the invention within a broad range of process conditions. It is my invention in the following claims to cover all such equivalent modifications and variations as fall within the true scope and spirit of my invention.

Claims (6)

What is claimed is:
1. A process for the recovery of uranium from uranium-containing ore which also contains molybdenum, comprising:
leaching said ore to form uranium and molybdenum values;
passing the leachate through an anion-exchange resin to capture said uranium and said molybdenum values;
eluting said resin with a salt solution containing an anion capable of replacing said uranium and said molybdenum values;
passing the eluate through a weak acid cationic resin in its hydrogen form to capture said uranium values;
eluting said cationic resin with an acid solution capable of replacing said uranium values to recover said uranium values free of molybdenum values; and
treating the eluate containing values to precipitate uranium therefrom.
2. A process as defined in claim 1 wherein said anion-exchange resin is eluted with a salt solution containing carbonate/bicarbonate.
3. A process as defined in claim 1 wherein said anion-exchange resin has quaternary amine functional groups.
4. A process as defined in claim 1 wherein said cationic resin is eluted with a solution of 4% HCl.
5. A process as defined in claim 1 wherein said cationic resin is eluted with a solution of 4% H2 SO4.
6. A process as defined in claim 1 wherein a major functional group of said weak acid cationic resin is a member selected from the group consisting of carboxylic acid, phenolic, phosphoric, and sulph-hydryl.
US06/311,579 1981-10-15 1981-10-15 Process for the separation and recovery of molybdenum and uranium from leach solution using ion exchange Expired - Fee Related US4375452A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4832924A (en) * 1986-12-26 1989-05-23 Doryokuro Kakunenryo Kaihatsu Jigyodan Process for producing uranium oxides
FR2687170A1 (en) * 1992-02-07 1993-08-13 Eurecat Europ Retrait Catalys RECOVERY OF MOLYBDENUM AND VANADIUM FROM USED CATALYSTS.
US20100084327A1 (en) * 2008-09-16 2010-04-08 Paul Goranson Recovery and precipitation of various elements and compounds
US20110024704A1 (en) * 2009-07-29 2011-02-03 Soderquist Chuck Z Compositions and Methods for Treating Nuclear Fuel
US9567237B2 (en) 2012-11-16 2017-02-14 Honeywell International Inc. Separation and recovery of molybdenum values from uranium process distillate
CN112827642A (en) * 2020-12-17 2021-05-25 南华大学 A kind of beneficiation, metallurgy and separation method of nickel molybdenum uranium ore

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3188169A (en) * 1962-09-20 1965-06-08 Kurt A Kraus Separation of metal values by cation exchange from concentrated perchloric acid solution
US4199470A (en) * 1977-05-13 1980-04-22 Koei Chemical Co., Ltd. Material for recovering uranium and method for recovering a uranium solution of high purity and high concentration, using the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3188169A (en) * 1962-09-20 1965-06-08 Kurt A Kraus Separation of metal values by cation exchange from concentrated perchloric acid solution
US4199470A (en) * 1977-05-13 1980-04-22 Koei Chemical Co., Ltd. Material for recovering uranium and method for recovering a uranium solution of high purity and high concentration, using the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Merritt, Robert C., "The Extractive Metallurgy of Uranium", Colorado School of Mines Research Institute, 1971, pp. 152-164. *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4832924A (en) * 1986-12-26 1989-05-23 Doryokuro Kakunenryo Kaihatsu Jigyodan Process for producing uranium oxides
AU600996B2 (en) * 1986-12-26 1990-08-30 Japan Nuclear Cycle Development Institute Process for producing uranium oxides
FR2687170A1 (en) * 1992-02-07 1993-08-13 Eurecat Europ Retrait Catalys RECOVERY OF MOLYBDENUM AND VANADIUM FROM USED CATALYSTS.
US20100084327A1 (en) * 2008-09-16 2010-04-08 Paul Goranson Recovery and precipitation of various elements and compounds
US20110024704A1 (en) * 2009-07-29 2011-02-03 Soderquist Chuck Z Compositions and Methods for Treating Nuclear Fuel
US8506911B2 (en) * 2009-07-29 2013-08-13 Battelle Memorial Institute Compositions and methods for treating nuclear fuel
US8636966B2 (en) * 2009-07-29 2014-01-28 Battelle Memorial Institute Compositions and methods for treating nuclear fuel
US9567237B2 (en) 2012-11-16 2017-02-14 Honeywell International Inc. Separation and recovery of molybdenum values from uranium process distillate
CN112827642A (en) * 2020-12-17 2021-05-25 南华大学 A kind of beneficiation, metallurgy and separation method of nickel molybdenum uranium ore

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